CN88102218A - The method and apparatus of the thermoplastic resin section bar that production strengthens with continuous fiber - Google Patents

The method and apparatus of the thermoplastic resin section bar that production strengthens with continuous fiber Download PDF

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Publication number
CN88102218A
CN88102218A CN88102218.7A CN88102218A CN88102218A CN 88102218 A CN88102218 A CN 88102218A CN 88102218 A CN88102218 A CN 88102218A CN 88102218 A CN88102218 A CN 88102218A
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China
Prior art keywords
fiber
web feed
groove
die head
equipment
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CN88102218.7A
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Chinese (zh)
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CN1017693B (en
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米歇尔·格兰密特
吉尔·科格内
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Arkema France SA
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Atochem SA
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/06—Fibrous reinforcements only
    • B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
    • B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
    • B29B15/10—Coating or impregnating independently of the moulding or shaping step
    • B29B15/12—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
    • B29B15/122—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/15—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor incorporating preformed parts or layers, e.g. extrusion moulding around inserts
    • B29C48/154—Coating solid articles, i.e. non-hollow articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/15—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor incorporating preformed parts or layers, e.g. extrusion moulding around inserts
    • B29C48/156—Coating two or more articles simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/06—Fibrous reinforcements only
    • B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
    • B29C70/16—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/40—Shaping or impregnating by compression not applied
    • B29C70/50—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC]
    • B29C70/52—Pultrusion, i.e. forming and compressing by continuously pulling through a die
    • B29C70/523—Pultrusion, i.e. forming and compressing by continuously pulling through a die and impregnating the reinforcement in the die
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/07—Flat, e.g. panels

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Textile Engineering (AREA)
  • Reinforced Plastic Materials (AREA)
  • Moulding By Coating Moulds (AREA)
  • Ropes Or Cables (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
  • Peptides Or Proteins (AREA)
  • Artificial Filaments (AREA)

Abstract

The present invention relates to produce the method and the production equipment thereof of the thermoplastic resin section bar that strengthens with continuous fiber.This method comprises that the fiber that will line up the glass rove of sheet shape in advance floods the feed glass rove in the die head with heading joint cover, and then will before entering the finished product shaping die, pass through a web feed zone earlier with the rove fiber of molten resin dipping, all fully flood as much as possible so that guarantee each root fiber of glass rove.

Description

The present invention relates to produce the method for the thermoplastic resin section bar that strengthens with continuous fiber and relate to the equipment of producing these section bars.The method comprises earlier floods the feed glass rove in the coating die head with heading joint cover, the component fibre of this kind glass rove is before entering the coating die head it to be arranged shape in blocks, in order to guarantee each root fiber of glass rove can both fully be flooded then, can lead to make its die head that is configured as final product before, with its whole web feed zone (bar feed zone) that passes through.The charging of coating die head is according to a conventional method, comes charging with at least one extruding machine.
As everyone knows, the available heat plastic resin comes the sheath glass rove, and for example United States Patent (USP) the 3rd, 834, No. 980.According to the sheath technology of routine,, use molten thermoplastic resin's charging of coming out and be coated with from above-mentioned right angle shield system with the die holder center of glass rove by heating.One glass rove is constituting by many continuous primary filaments.
In the sheath technology of the section bar that described production strengthens with continuous fiber, normally many strands of glass roves are wound in a kind of form of yarn bundle with spool.Under these conditions, two insurmountable main difficulties have been run into.First point is the core that is difficult to be impregnated into the yarn bundle, also is difficult to thermoplastic resin is evenly distributed on the every primary filament.Second point, also because first kind of difficulty causes promptly between the fiber of finished product gas enclosure is arranged, this kind gas enclosure is the root that mechanical performance produces defective.
According to United States Patent (USP) the 3rd, 933, be actually mutual rectangular plate washer owing to be provided with two in the die head No. 726, so can flood by the glass rove that one is independent at dipping.Therefore, when flooding in this way, this a glass rove just direction in a plate washer scatters and floods, and the rightabout in second plate washer is extruded it again then.This kind device has two shortcomings: first shortcoming is to flood independent glass rove; Owing to be provided with this kind plate washer, so each root fiber of the glass rove of impossible dipstick shape, because the glass rove of sheet shape can not make fiber break into bundle filling the rotation of carrying out about 90 degree in the die head of plastic material, second shortcoming is the position that occurs in the plate washer in the equipment; All plate washer all is to be placed in the die head, and this just makes glass rove stand twice directly extrusion in the plastic material of fusion, therefore makes the fiber that comes out from die head produce powerful pulling force, thereby causes fiber breakage.Therefore, under these conditions, the impregnating effect of fiber is unsafty, and the flexural property of finished product is also very poor.Equally, also very poor with the enhancing efficient that coefficient ε represents, this coefficient ε is no more than 0.25.
Identical with above-mentioned patent, United States Patent (USP) has been narrated for the 4th, 312, No. 917 and has been filled in the die head of molten plastic material, to the coating that indivedual glass rove carried out.Except above-mentioned shortcoming, this kind technology also has another kind of shortcoming, because the glass rove of Yin Ruing is reciprocally then to enter die head from the outside, and in fact meet at right angles with the die head axis, will produce the new stress and glass rove is intertwined since second block of shelves baffle of fractureing like this, particularly because the cooled glass rove can make molten resin gelling suddenly in its surface.
Method of the present invention at first is the die head that glass rove is passed coated fiber, and it is not that glass rove is introduced with the form of yarn bundle, but each strand rove is opened, and each root fiber of each strand rove is scattered abreast.In such cases, rove just becomes the sheet shape yarn be made up of side by side single continuous fiber one by one or the form of band shape yarn.In order to produce this kind fiber is that the also while that is arranged in a row is again the glass rove that scatters, glass rove is passed at least one plate washer of the first web feed zone, after Wei Wei in the glass rove is scattered, be introduced into again in the coating die head of the thermoplastic polymer that fusion is housed.Then with formed shape yarn or band shape yarn, with thermoplastic resin impregnated, and before entering shaping die, with new web feed zone that is made of plate washer of they introducings, in fact these plate washers are parallel to each other with the plate washer in first district.In this system, parallel to each other and by at least two facing to the plate washers of placing through the thermoplastic resin impregnated sheet shape yarn of fusion or band shape yarn.Under these conditions,, make between the resin infiltrated fiber of molten condition, so that make it arrive the other one side of fiber all extruding on a surface of first plate washer with thermoplastic resin impregnated fiber.When above-mentioned plate washer of fiber and opposite that has flooded resin contacts, will produce a kind of opposite effect.The web feed system that adopts before and after sheath sheet shape yarn or band shape yarn can make each root fiber flood, thereby make resin homogenizing and distribution preferably on fiber, and in fact all remove the air that contains in the glass fibre.
Present technique can make the fiber in whole glass roves scatter at the first web feed zone, and it is arranged in parallel to form sheet shape yarn.Still untreated fiber just enters the dip-coating die head so these have been arranged, at this moment it all is separated from each other that fiber is actually every, therefore just make every fiber can both obtain good dipping, and any danger that fractures can not arranged before the district that enters the second web feed zone.
Accompanying drawing can illustrate the present invention preferably.Fig. 1 illustrates a complete set of equipment of producing section bar.This complete equipment comprises the web feed system of representing with 1 that the glass rove fiber can be scattered.What represent is the coating die head with 2, be connected with extruding machine before the web feed system that is positioned at impregnation of fibers 3, but this extruding machine does not illustrate on figure.At last, what represent is shaping die with 4.Be made up of a groove with the 1 web feed system of representing, glass rove " a " then stretches by this groove.This groove can have any geometry, but is preferably the cross section with rectangle, so that make glass rove line up the form of sheet shape yarn or band shape yarn easily.The inlet of groove can be tubaeform, so that make the smooth access arrangement of glass rove.In this groove, has a plate washer " b " at least, the direction deflection that glass rove is stretched.Therefore the axis normal that in fact this plate washer stretches with glass rove also is rectangular with groove, thus when glass rove through out-of-date, they just are close on the described plate washer, thereby the fiber of forming each strand glass rove is kept flat.Usually there is a plate washer just much of that, if but when wish forming fibrous shape yarn by many strands of glass roves, preferably adopt the web feed system that several plate washers are arranged.In order to improve fiber impregnation effect subsequently, a vacuum deflation pipe " c " can be set, remove the air that contains in the glass rove as much as possible.Simultaneously, also recommend to use a kind of heating system.Coating die head 2 is die heads of a kind of molten polymer coating of a kind of common usefulness as you know continuous fiber.This is a kind of die head with heading joint cover.It can come coated fiber with molten thermoplastic material.
The part 3 of this equipment is second web feeding system, usually be heated the temperature that equals at least the thermoplastic resin fusion, this system mainly is made up of a groove " d ", and this groove is in order to receive the fiber through the resin coating of fusion on the extended line of coating die head.This groove comprises at least two plate washers " e " and " f ", and these two plate washers are actually the axis normal with groove, otherwise is exactly with the axis normal of stretching coated fiber and faces toward mutually, thereby, when stretching, make the surface of each dip-coating all can be alternately stressed.As mentioned above, these plate washers are actually parallel with plate washer " b ".At last, the fiber of process dipping is being cooled when equipment comes out by behind the shaping die 4.This kind shaping die is exactly any extrusion molding system the sort of shaping die commonly used, makes the net shape that die head provides that has of product.According to known technology, should be realized that geometry according to die head, can make senior section bar, or foolproof web, people can be cut into particle with this kind web, so that subsequently by using other process technologies to be made into other products.
Fig. 2 is the profile that the part 2 of the Fig. 1 that is coated with die head is described.This figure illustrates a kind of well-known die head, and it can be coated with the glass rove fiber of lining up sheet shape yarn.An extruding machine 5, this figure is not shown, and by feed well 6 and 7 thermoplastic resins to groove 8 supply fusions, groove 8 represents with the square-section that in the drawings the sheet-shaped fiber yarn just draws in this pipe.Feed well 6 and 7 is arranged to and can makes molten thermoplastic material be distributed to two the wideest surfaces that face toward mutually of sheet-shaped fiber yarn at least.
Fig. 3 explanation is used for constituting the profile of the part 3 of the second web feed system.This figure is specially adapted to the present invention, and according to this figure, plate washer curves with the true form of groove, and these two plate washers sinusoidally form waveform between coating die head exit and shaping die.According to this system, this is a metal derby, preferably heats, and passes the groove of the coil form of a sine in this metal derby, the groove of this coil form has at least two parallel plate washers that face toward mutually, uses the expression of sinusoidal peak " f " and ebb " e " respectively.
Just can understand in the web feed system of Fig. 3 referring to Fig. 4, be close to the glass rove fiber " g " that is arranged in a row on the sine curve peak, be the thermoplastic resin " h " that how to force fusion passes in the middle of them, thereby improve their coating effect.
The method according to this invention can be made the section bar that the continuous fiber produced with any extrudable thermoplastic polymer or copolymer strengthens.The most frequently used polymer and copolymer comprise: polyolefin, for example polyethylene or polypropylene, vinylaromatic polymer and copolymer thereof, for example polystyrene and acrylonitrile-butadiene-styrene copolymer, fontanel ethene polymers, for example polyvinyl chloride and Kynoar, polyamide, for example polyamide fibre 6,11,12,66,610, polyester, for example poly-to benzoic acid dioctyl phthalate second fat and poly-to sour dioctyl phthalate fourth fat, poly--(ether-amide) block copolymer, polysulfones, polyether sulfone, poly-charcoal acid fat, polyether-ketone, polyphenylene sulfide, PEI, polyphenylene oxides, polyphenylene oxide or its mixture.
Extrudable thermoplastic polymer strengthens with inorganic or organic continuous fiber.For example, fibre glass roving, silicon rove, carbon rove or fragrant acid amides rove.
According to the shape of die head, just can use prepared section bar through strengthening.They can also use as intermediate product in methods such as injection moulding, compression moulding, injection moulding-compression moulding, extrusion molding in batching or after being processed into particulate.
Following example explanation the present invention, but can not limit the present invention.
Example 1:
Use is according to the equipment of Fig. 1, and its specification is as follows:
-web feed zone 1:
-length: 60 millimeters
-width: 100 millimeters
-die slot: 3 millimeters
Inlet is widened, and the convex plate washer is high 10 millimeters
-feed die district 2:
-length: 90 millimeters
-width: 100 millimeters
Article two, the feed well diameter is respectively 10 millimeters
Die head district outlet die slot: 3 millimeters
-charging: 30 mm dia extruding machines
-spiro rod length: 22 times of diameters
Bar shaped feed zone 3:
-length: 200 millimeters
-width: 100 millimeters
The sine curve web feed zone at-3 peaks
-peak-to-peak amplitude: 40 millimeters
-die slot: 3 millimeters
District 4 is shaped:
-5 casement heads, aperture: 3 millimeters
100 millimeters of-length
-width: 100 millimeters
This equipment is used for producing use 50%(weight) polyamide fibre 11 bands of E glass 2400tex glass fiber rovings filling.
Draw speed: 3 meters/minute
The temperature in each district is:
Distinguish 1:200 ℃
Distinguish 2:230 ℃
Distinguish 3:230 ℃
Distinguish 4:210 ℃
Example 2:
With the equipment of example 1, make and use 39.3%(weight) the width made of the E glass 2400tex glass fiber rovings polyamide fibre 6 of filling be that 10 millimeters and thickness are 3.5 millimeters web, but be shaped distinguish 4 have following specification and and then this district one cold shaping machine is arranged:
The import square-section, wide: 100 millimeters, thick 3 milli degree
The outlet square-section, wide: 10 millimeters, thick 3.5 millimeters
Length: 100 millimeters
Draw speed: 3 meters/minute
The temperature in each district is:
Distinguish 1:220 ℃
Distinguish 2:280 ℃
Distinguish 3:280 ℃
Distinguish 4:260 ℃
The web modulus in flexure of measuring is 24500 MPas
Coefficient ε: 0.85
Coefficient ε measures according to law of mixtures:
E＝εEf+Em（1-vf）
In the formula: Ef=fiber young modulus
Em=base-material poplar is a modulus
Vf=fiber volume umber
The experiment value of E=modulus in flexure.
Example 3:
With example 1 equipment, make and use 40%(weight) the band made of the polyamide fibre 12 of E glass 2400tex glass fiber rovings filling.
Draw speed: 3 meters/minute
The temperature in each district is:
Distinguish 1:220 ℃
Distinguish 2:260 ℃
Distinguish 3:260 ℃
Distinguish 4:240 ℃
Example 4:
With the equipment of example 2, make and use the 28%(volume) E glass 2400tex glass fiber rovings fill and contain the polypropylene web of 3% polyacrylic usefulness maleic anhydride grafting.
Draw speed: 3 meters/minute
The temperature in each district is:
Distinguish 1:240 ℃
Distinguish 2:260 ℃
Distinguish 3:260 ℃
Distinguish 4:240 ℃
The modulus in flexure of measuring is 15400 MPas
Coefficient ε=0.78
Example five:
With the equipment of example 1, but long 200 millimeters in district's 4 usefulness, five casement heads in single outlet die head alternate area 4 that die head exit wide 100 millimeters and die slot are 0.7 millimeter are made and are used 40%(weight) the polyamide fibre 6 of E glass 2400tex glass fiber rovings filling make sheet material.
Draw speed: 1 meter/minute
The temperature of each is:
Distinguish 1:220 ℃
Distinguish 2:280 ℃
Distinguish 3:280 ℃
Distinguish 4:275 ℃

Claims (8)

1, the method of the thermoplastic resin section bar that production strengthens with continuous fiber, this method is included in the die head that is coated with continuous glass rove fiber and is coated with thermoplastic resin, it is characterized in that, before coated fiber, the fiber of glass rove is scattered, become sheet-shaped fiber, these fibers promptly are arranged in a row behind at least one baffle plate by the web feed zone abreast, its feature also is, after with the fiber coating, to pass the second web feed zone of forming by the plate washer of at least two parallel placements that face toward mutually with the fiber of molten resin dipping again, force between the resin infiltrated fiber.
2, according to the method for claim 1, the plate washer that it is characterized in that two web feed zones all is parallel.
3, according to the method for claim 1 or 2, it is characterized in that these plate washers in fact with equipment in the axis normal passed through of continuous fiber.
4,, it is characterized in that the first web feed zone is heated according to the method for any one claim in the claim 1 to 3.
5, the equipment of the thermoplastic resin section bar that production strengthens with continuous fiber, this kind equipment mainly is made up of die head and a shaping die of a coating continuous fiber, it is characterized in that, before the coating die head, by a web feed system of forming by a groove, this groove has at least one plate washer that is actually with the axis normal of described groove, it is characterized in that, between coating die head and shaping die, a second web feed system that is made of a groove is arranged, this groove is positioned on the extended line of coating die head exit, has the plate washer of at least two parallel placements that face toward mutually, and in fact with the axis normal of described groove.
6, according to the equipment of claim 5, the plate washer that it is characterized in that two web feed systems all is parallel.
7, according to the equipment of claim 5 or 6, it is characterized in that the second web feed system is made up of a metal derby, in this metal derby, pass the groove of the coil form of a sine, the groove of this coil form has at least two parallel plate washers that face toward mutually, represents with sinusoidal peak and ebb respectively.
8,, it is characterized in that the first web feed zone is equipped with a heater according to the equipment of any one claim in the claim 5 to 7.
CN88102218A 1987-04-09 1988-04-09 Process and apparatus for production of profiles of thermoplastic resin Expired CN1017693B (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8704996 1987-04-09
FR8704996A FR2613661B1 (en) 1987-04-09 1987-04-09 PROCESS FOR PRODUCING CONTINUOUS FIBER REINFORCED THERMOPLASTIC RESIN PROFILES, APPARATUS FOR OBTAINING SAME

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Publication Number Publication Date
CN88102218A true CN88102218A (en) 1988-11-02
CN1017693B CN1017693B (en) 1992-08-05

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EP (1) EP0287427B1 (en)
JP (1) JP2537152B2 (en)
KR (1) KR930000743B1 (en)
CN (1) CN1017693B (en)
AT (1) ATE65457T1 (en)
CA (1) CA1326748C (en)
DE (1) DE3863822D1 (en)
DK (1) DK173248B1 (en)
ES (1) ES2006612A6 (en)
FI (1) FI92985C (en)
FR (1) FR2613661B1 (en)
PT (1) PT87199B (en)

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PT87199A (en) 1988-05-01
US4957422A (en) 1990-09-18
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FI92985C (en) 1995-02-10
CN1017693B (en) 1992-08-05

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